Pbocess of treating matebial with aas ob vapob



F. L. SLCUM. PROCESS 0F TREATING MAIERIAL WITH GAS 0R VAPOR Mwucmon msoszPLzi. |911.

1,315,582. n latemedsepn 9, 1919.

2 SHEETS-SHUI l.

F. L. SLOCUM. PROCESS 0F TREATING MATERIAL WITH GAS 0H VAPOR- APPucAIloNmin s:P1.2|. 1911.

l ,31 5,532. PutentedSept. 9, 1919.

2 SHEETS-SHEET 2.

anotan,

FRANK L. SLOCUM. 0F PITTSBURGH. PENNSYLVANIA.

PROCESS OF TREATING MATERIAL WITH GAS ON VAP'OR Specification of LettersPatent.

Patented Scpht).f 1919.

Application filed September 21. 1917. Serial No. 192,483.

To ull whom Ait 'muy concern.'

lie it known that I` Fassa L. SLoCUM, a.

citizen of the linited States. and resident.V

otl ltlsburgh. in the county of Allegheny and State of Pennsylvania.have invented a new and useful improvement in Processes ot' TreatingMaterial with (ias or Vapor; and l do hereby declare the following to bea fulLfcIear. and exact. description thereof.

My invention relates to the treating of a solid with gases or valmrsandpartictllarly contemplates the combination of n series or several seriesof steps in one continuous pro-4 gas on a carbid under stl'itabneonditions,

and second, the formation o'f ammonia and its compounds by means of theaetioirof water or steam on the nitrogen containing material. 'lheresidual material. ma) then be ealeined il' desired. ll of saiddescribed steps or processes may be carried on in close succession alnlin the same apparatus.

lt is of special advantage that the steps in the production of annnouiaaml its oompounds. for example. be carried on iu close succession andi.u the same ap mratns since, by so doing. a great saving o time.results. deterioration of the material is prevented and great economy ofheat is etlected.

Further. the reactions that take. place. bei tween steam and water andtho nitrogen containing material may be much more easily regulated.since the n naterial may. for example. be. cooled to laniz'hdosn'ct'ttemperature in au atmosphere of steam or nitrogen or kept. at adesired'tenmerature in an atmosphere of steam or raised through anydesired tenipta'ature range in an atna. :plaire of stema, nitrogen orany desired gas lor vapor au'ordiag to the particular result desired.'lhe sta'ies of reactions may be intlneneed in any desired way .bytheemploymentl of a suitable catalyst or mixture of catalysts,

For the purpose of clear illustration ot' a preferred manner of carryingont my iurproved process, I will describe a form ot' ap paratus whichmay be employed to advantage in carrying out the process and will thendescribe the several steps 'of the process as they may be carried out insaid appa ral-us. It is to be understood, however, that. the apparatushere referred to is described merely for convenience to make clear tothose. skilled in the art one means by which the )recess may beadvantageously and practica ly carried out.

In the. accompanying drawings which illustrato such form of a paratus.

Figure 1 is a lougitucinal sectional view of a furnace for carrying outthis process;

Fig. 2 is a transverse sectiohal view ot the furnace on t-he line 2 2,l"ig.'1;

Fig. 3 is a longitudinal sectional view ot one of a number of trays inwhich the material may' bc held in the furnace;

Fig. 4 is a. fragmentary' plan view ot' said tray; and

Fig. 5 is a perspective view of a charging rack or carrier for carryingthe trays into and out of the heating chamber of the furnace, as well assupporting them within the.

.furnace during the several reactions on the material.

In the embodiment. of a ipnratus herein selected for illustration andreferring particularly to Fig. l of the drawing, the uumeral 1 indicatesthe furnace in general. This furnace may be of the regeneratm' form' andma) comprise a plurality ot' heating chambers. one of which is indicatedat 2, said chambers cach having end doors :l at either end respectively,and a top l. in which is mounted an outletfpipe b v which the gases orvapor products of the reactions within the heating chamber may bedischarged. .,In' the construction here shown.' a covered trapor've-sscl 6 is provided which is )referably filled with oil or othersuitable tlmd to the level above. the discl rrge end 7 of the outletpipe and n second illischarge pipe H enters said trap and terminatesabove the. level o'f the 'liquid therein, whereby the 'desired gaseousproduct.l V of. the heating chamber may be"conducted to a suitablecontainer.

Extending from one end of the heating llll chamber is a supportingplatform 9 which is 'flush with th'e Hoor of the chamber and forms aSupport and guide as desired for the charging rack or ca'ge by which thematerial 1s charged into and'withdrawii from the heating chamber.

In order that the gases or vapors with which the material such as carbidis to be treated, may have free access to all parts of said material, itis desirable that the material or carbid be distributed in dividedmasses within the heating chamber, the material being preferably spreadin comparatively thin and separated layers so that thel gas or vapor mayact quickly upon th'c same.

To this end, therefore, I provide a suitable form of charging rack orcage so constructed and arranged as to support thereon more or lessshallow' trays within which tluelnaterial is.

contained. In the form of thisinvcntion here particularly illustrated,this charging rack or cage may comprise a suitalde frame work consistingof a skeleton body or frame. having mounted thereon` sever-.d uprights11, which are bollini together on each side of the .rack by a pluralityof longitudinal stringcrs er side frame members 1Q and these side framesuml the rack so formed are connected and strcngthelnal by cross memberslit at top and bottom, see. Fig. 'lhe longitudinal stringers or framemembers l2 are preferably 'ol' angle iron construction, the verticalflanges 1l of which are riveted or otherwise fastened to the uprightframe. members 1l Aand the laterally extending flanges l5 of which formsupports for the tray containing material to be treated. These chargingracks or ages may lavprovided with suitable rollers lt by which the rackis easily run into and out of the heating chandler.

Referring now to Figs. 3 and l, particu-` larly. the. trays t'orsupporting the material wit lin the heating chamber. consist. prefer.ably of more." or less shallow pans 1T., the bottom and side walls ofwhich are perforated throughout: to permit of free. access of gas orvapor to thematerial contained |here in; ln order that the material,il'in tlnform of more or lcSr' small particles, may not fall through the.perforations ol the tray. each tray may, if necessary, he provided witha layer 18 oil meshed material. such as wire mesh screen, which'overlies the perfo- Ipitted bottoml of the tray and may. if necesvsal'v, be. cxtcndet'l.4 npdver the perforated the sido walls' thereof sidesof the tray.

.During thc trtaltluent, ofthe material such' as carbid while su iporledon the tray within tha heating chamber, reactions occur which nuiyeause.the swelling pr expanding of the material. ln order Io allow l'orsuc.h.s\\ell log or expansion 4witlamt'in'ury to tlie 't`r1\y. '.,aretaredor slanted "thereon, it -will be seen that said trays areseparated, one from the other, whereby the.

"as or vapor with which the heating chamlier 1s charged may have freeaccess to every part of the material 1n the trays and masmuch as thismaterial is more or less thinly spread out 1n said trays, the gas orvapor will readily permeate and saturate the material.

The outlet pipe l1 leading from the heating chamber n'iay be providedwith a valve or other controlling means lt), by which the discharge ofthe products of reaction in vapor or gaseous form may be. controlled.

'lhe nitrogen or other gas or the. steam or vapor may be supplied to theheating chambcr or chambers.

ln Fig. 1, the charging rack is indicated in dotted outline as withdrawnfrom the heating chamber and resting upon the platform t). Any suitableform of ram or other means (not shown)V may be employed for shifting thecharging rack into and ont ot' the. heating chamber.

'l'he particular apparatus herein described forms lthe. subject-matterol' my rompanion application- Seriai .\`o. ltlLJSz! liled on the 'Jlstday of`Septemlxa', ltll.

ln describing the manner of using the apparatus heretofore referred to,l will use the treatment of calcium carbid with nitrogen to formcalciluna'arbon-.nitregen conipounds and the treatment of the compoundso formed with steam for the production ol` ammonial and ammoniumcondannata4 and calcium com munds aml free carbon residues a's a typicaillustration of my improved prmfess.

'l`l|e. process may be carried out in d etail in the following manner:lhe closed hea ing chamber or oven, containing thi` ear-bid, tilled withnitrogen gas under slight pressure by direct comxection with thenitrogen steam, the nitrogen is shut oli' and steam at propertemperature and pleasure `is admltled 'by which 'the material is'further cooled. if |uiecima|'y`,`to the.temlxeratnre best suited t'orfurther treatment. ln carrying 'as slanvnin lfig. 1.5 sconttheprimissdescribed in the -Taylorr ilu loo llo`

lll',

Knapp applicattm, Serial No. 191,185, tiled September 12.1,"1917, it isnecessary to ,cool the oven and the material contained therein to apoint below 2550" C. before admitting steam. Y

ln carrying out my process 1 need cool the heating c mmbers or ovens andthe material therein, only to approximately 450 C. or the temperaturemost suitable for the. conversion of the nitrogen contained in thecompound into ammonia and its compounds. The temperature nniintainedduring the evolution of ammonia. or ammonium ,compounds may be withinthe range below (300 C. The treatment with steam is preftrays emptied.retilled with carbid and' after charging in the oven the cycle begins lagain; or the heat is tirst raised to approximately 850" l. to removeall moisture and most of the carbonie acid gas from any calciumcarbonate previousl formed, thus calcining the residual pro( uct.

From the above described process it will be seen that the desired finalproduct may be produced by a continuous serie-s of steps vin asingltapparatus and in the most ellicient and economical manner inpoint. of time. possible deterioration of the. material and in a mannerpermitting close regulation of the. conditions under which the severalsteps ol' the. process are performed.

While l have herein descril'ied the particular manner of carrying ont.my improved process and the particular order in which the steps may beperformed, likewise a particular form of apparatus in which the processmay be carried on, it is to be Illldcrstood that such specilicdescription is' merely illustrative and that the details hereindescribed can be. varied to any dclsired and practical extent wit-hinthe scope of the appended claims.

Having described the invention what is claimed is:-

l. lhe process for the production of ammonia aml its compound from acarbid and nitrogen which comprises carrying ont. all of the necessaryreactions in a continuous series of operations and in one apparatus.

2. lhe process for the production of ammonia and its compounds, whichcomprises ltreating calcium ca ifiid nith .nitrogen gas. subjecting :hisn ltrlhed material to the aetion of stt-.fm and recovering the ammoniaevolved in a series of operation.` in llnsame apparat-us.

3. The process for the production ol' ammonia amt its compounds and thecaleining of the residual material. which comprises treating a, carbidwith nitrogen gas. subjecting this nitritied material to the action ofsteam until the ammonia formation is .substantially completo whilerecovering the evolved ammonia and then raising the tcmperat-ure. of themass to a point suilicient to expel all of the water and substantiallyall of the carbon dioxid from the residual material.

4. 'lbe process for the production of ammonia and its compounds aml thecaleining of the residual material which comprises the following stepsor react-ions in a continuous series of operations, namely, treating acarbid with nitrogen gas attem|uratures suitable for the absorptionofthe nitrogen. cooling the nitrified material to a suitable temperatureand treating with steam to cause. the production of annnonia and itscompounds while collecting the evolved amlnonia and its eompoumls. andraising the. temperature ol' the furnace aml itsI contents totemperatures suitable for expelling the wate and substantially all thecarbon dioxid from the residue.

.'i. 'l`he process for the production 'ol ammonia and its compounds andthe ealcining of the residual material, which comprises the followingsteps or reactions in a continuons series of operations. namely;treating a carbid with nitrogen gas at a tempel ature not in excess of1000" t.. cooling the ntrilied material, treatingthis nitrilied materialwith .steam below H00" (l. while. recovering the evolved aunnonia. andraisingr the te||i|a.r:|t.|li'e of the furnace aml its contents toapproximatelv H50 whereby the water and substantially all the carbondioxid are expelled from the residue..

(i. 'l'hc process for the production of ammonia and its compounds. whichcomprises the following steps or reactions in a continuons series ofo|wrations, namely. treat-- ing a carbid alone or a carbid mixed with acatalyst with nitrogen gas or nitrogen containing catalytic vapors org-:scs at tcmpcratures .suitable for the absorption ol' the gas by thecarbid. cooling the nitrllied material to a temperature suitable l'ortreating it; with steam, and treating this nitrified material lwithstealn at lemlwratures suitable for prtxiucing ammonia and its compoundswhile reeovering the evolved products.

7. 'lhe irocess for the production of ammonia am its compounds and thecalcining of the residual material, which comprises tno llu

the. following steps or reactions in a. continuous series of operations,namely, treating a carbid with nitrogen gas at-a temperature not inexcess of 1000 C., cooling the nitritied material to substantially 450C., and' treating this nitrified material with `steam between 450 C: and000 C. while steam until the evolution of ammonia is completed.

il. The I )rocess for the production of ammonia which comprises heatinga carbid in au atmosphere of nitrogen gas at a temperutllre necessary tocause substantial saturation of the carbid with the nitrogen. andtreating the nitrilicd material with steam at. atmospheric pressureuntil the evolution of ammonia is completed.

l0. 'l`he process for producing ammonia aml calciuing the residualmaterial which comprises heuting`tbc carbid in an atmosphcre otnitrogengas` cooling the mtrilied material b v means ol` the nitrogen gas,subjet-ting the cooled mass to the action of steam until the ammoniaformation is substautiall \l complete, aml raising the temperature ofthe mass to a point sutlicient to expel all the watel' and.substantially all the carlton tliosid from the residual material.

ll. 'l`he process for the production of am monia winch comprisestreating a carbid with nitrogen gas in the presence ol' heat. until theycarbid is substantially saturated with said gas` cooling the nitriliedmaterial with steam. uml eontiutting the treatment with steam until theevolution of ammonia is substantially complete.

l2. 'lhe process for the production of ammonia which comprisescolnhining the following steps or reactions in a continuons series ol'na-rations, namely` t renting a carbid with nitrogen gas at temperaturessuitable to cause the absunplion of the gas. cooling the 'nitriliedmate-rml by means of nitrogen to temperatm'es suitable for tieatmeut ofthe. material withsteam, and treating this uitrilied material with steamat. temperatures suitable for the production of ammonia and its`eompoumls while recovering the evolved products. i

t3. Theproeess for the production of ummonia. which 'comprises combiningthe. following steps or reactions in a continuous series of openttions.namely, treating a ear bid with nitrogen gas at a temperature not inexcess of 100()o C., cooling the nitrilied material by means of nitrogento substantially 450 C., and treating this nitrited material with steamtween 450 and 000" while recovering the evolved ammonia.

14. The )rocess for the production ot' ammonia anti ammonium compounds.which comprises combining the following steps or reactions in a,continuous series ot' operations, namely, treating the carbid mixed witha catalyst with nitrogen gas at tcmperatures suitable to cause theabsorption ot' the. gas, cooling the nitriticd material by means ofsteam to a temperature suitable lor evolution of ammonia and itscompounds b v said treatment with steam. and continuing the treatmentwith steam until ammonia and its compounds have been evolved to the desired extent while recovering the evolved produrt.

l5., The process t'or the production ot' ammonia which comprisescombining the t'ollowing steps or reactions in a continuous series ofoperations. namely` treating a car bid with nitrogen gas at atemperature not in excess of 1000 cooling llle nitrilietl material bymeans of steam to substantially 450 (1.. and continuing the treatmentwith steam between 450" aml t300" while recovering the evolved ammonia.

10. The prtx'ess for the production of ane lnonia. aml the calcining ofthe residual mate-rial which comprises treating a carbid with nitrogengas, cooling the nitritied material by further treatment with nitrogengas. trea.ting'tlu cooled material with steam until the auunoniaform-ation is substantialbv complete while recovering the evolvedammonia. then raising the temperature of the mass to a point sntlcicntto expebull thc water and substantially all the carbon dioxid from tht`residual material.

17. 'lhe process for the production ot' ammoniak and the calcining ofthe residual material which comprises treating a carbid with nitrogengast ctmling the uitrilied material b v means of steam to a point atrwhich decomposition of ammonia will not tale` place. continuing thetreatment ot' strait; until the ammonia formation is suhstantialbvcomplete while. recovering the evolved animonia and then raising thetemperature ot the mass to a point sutlicient to expel all the water andsubstantially all carbon dioxtl t'rom the residual nlateriaL lntestimony whereof. I the said l"u.\.\a I.. Swen. have hereunto set myhand.

FRANK L. SLQCUM.

llitncsses:

Cnaumzs R. VVmon'r, Jr., Fwru R. ConNwaLL.

llt)

Correction in Letters Patent No. 1,315,532.

It is'hereby oertied that Letters Patent No. 1919, upon the applicationof Frank L. Slooum, of Pittsburgh, Pennsylvania, for an improvement in*"Pxocesses rif-"Treating Material with Gas or Vapor, were issued to theinventor, said Slocum,

as sole owner of said invention,

have been issued to Jams Henry Reid, of

erroneously whereas said Letters Patent should Pittsburgh, Pennsylvania,as assignee of the entire interest 'in said invention, as shown by therecord of assignments in this otiice; and that the said Letters PatentShould be read with-thiscorreotion therein record of the case in thePatent Oce.

that tne same may'oonform to the sighed and mnd this 25th-dey orNovember, A. D., me. [gwn M. H, CoULsToN. Acting Commissioner ofPatents.

1,315,532, granted September 9,

Certificate of Correction,

lt is hereby -certified that Letters lntent No. 1,315,532, grantedSeptember 9, 1919, upon the application of Frank L. Slocum, ofPittsburgh, Pennsylvania, for an improvement in Processes of TreatingMaterial with Gas or Vapor, were erroneously issued to the inventor,said Slocum, as sole owner of said invention, whereas said LettersPatent should have been issued to International Nitrogen Uompanfy, aCorporation of l/elewwe, said corporation being assignee, by 'memeassignments, of the entire interest in said invention, as shown by therecords of assignments in this oioe; and that the said Letters Patentshould be read with this correction therein that the same may conform tothe record of the case in the Patent Ofce.

This lCertificate supersedes Certificate of Correction isslied November25, 1919.V

signed and ned his 25th day of April, A. D.., 1922.

{me} KARL FENMNG,

`Acting Uommasmwr of Patents.

